CN113044883B - Preparation method of three-dimensional embroidered spherical tungsten disulfide electrode material - Google Patents
Preparation method of three-dimensional embroidered spherical tungsten disulfide electrode material Download PDFInfo
- Publication number
- CN113044883B CN113044883B CN202110277837.0A CN202110277837A CN113044883B CN 113044883 B CN113044883 B CN 113044883B CN 202110277837 A CN202110277837 A CN 202110277837A CN 113044883 B CN113044883 B CN 113044883B
- Authority
- CN
- China
- Prior art keywords
- solution
- washing
- electrode material
- spherical
- embroidered
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a preparation method of a three-dimensional embroidered spherical tungsten disulfide electrode material, which comprises the following steps: respectively dissolving tungsten hexachloride and methylimidazole in a methanol solution, mixing the two solutions, standing and collecting light blue precipitate. Dispersing the precipitate in ethanol solution, adding thioacetamide, stirring, transferring to a hydrothermal kettle, and carrying out hydrothermal reaction for 12-72h, wherein the solvent thermal temperature is controlled to be 180-240 ℃; after the reaction is finished, washing and freeze-drying a reaction product to obtain a black three-dimensional embroidered spherical tungsten disulfide material; the obtained electrode material has good structural stability and higher capacity.
Description
Technical Field
The present invention relates to WS 2 The technical field of nano material preparation, in particular to a preparation method of a three-dimensional embroidered spherical tungsten disulfide electrode material.
Background
The two-dimensional transition metal sulfide is of a layered structure and exists in a form of X-M-X, and chalcogen element atoms are separated by transition metal atoms to form a sandwich structure to isolate the two-dimensional transition metal sulfide in two hexagonal space layered structures. The overall structure of the two-dimensional transition metal chalcogenideIs quadrilateral or hexagonal. WS 2 The transition metal chalcogenide has a hexagonal-phase graphene-like laminated structure with large interlayer spacing
The unique layered structure and the larger interlayer distance are beneficial to the intercalation and deintercalation of sodium ions, and are potential sodium ion battery negative electrode materials. But the material has a larger volume expansion problem in the charging and discharging process, so that the cycling stability of the material is poor. And the material itself has poor conductivity, which is not conducive to electron transport. The conventional solution to the problem of volume expansion is to synthesize a composite material with carbon as a matrix, relieve the stress generated in the volume expansion process of the composite material and enhance the conductivity of the composite material.
According to literature reports, the electrochemical stability of the composite material can be effectively improved by synthesizing the composite material with the carbon material as the matrix. The carbon material is beneficial to electron transmission, and can relieve stress generated by volume expansion of the electrode material in the charging and discharging processes, so that particle agglomeration is prevented. But due to the lower theoretical capacity of carbon, compounding it results in a reduction in its overall capacity. Therefore, it is a matter of consideration that how to improve the structural stability of the material itself, and thus the electrochemical performance, is required.
Disclosure of Invention
The invention aims to provide an embroidered spherical WS with good structural stability and higher capacity 2 A preparation method of the electrode material.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the method comprises the following steps: adding 0.3965-1.965 g of methylimidazole into 20-100 mL of methanol solvent, and stirring and dissolving to obtain a solution A;
step two: adding 0.793-3.96 g of tungsten hexachloride into 20-100 mL of methanol solvent to ensure that the molar concentration of the tungsten hexachloride is 0.1mlo/L, and stirring until the tungsten hexachloride is dissolved to obtain a solution B;
step three: pouring the solution B into the solution A to obtain a mixed solution C, stirring until the mixed solution C becomes a blue turbid solution, and standing for 12-72h;
step four: centrifugally washing the blue turbid liquid to obtain a blue precursor;
step five: dispersing the precursor in ethanol solvent, and then adding 0.7511-3.75 g thioacetamide for stirring; transferring the solution into a hydrothermal kettle, sealing the hydrothermal kettle, putting the hydrothermal kettle into a homogeneous reaction instrument, controlling the solvothermal temperature to be 180-240 ℃, reacting for 12-72 hours, and naturally cooling to room temperature after the reaction is finished;
step six: opening the reaction kettle, taking out the product, repeatedly washing the product by adopting absolute ethyl alcohol and deionized water in sequence, centrifugally separating the product, and drying the product in a freeze dryer with the temperature of between 40 ℃ below zero and 70 ℃ below zero and the vacuum degree of between 10 and 40Pa for 8 to 12 hours to obtain the black embroidered spherical WS 2 A material.
The volume ratio of the methanol solution obtained in the step 1 and the step 2 is 1:1.
the mass ratio of the tungsten hexachloride to the methylimidazole added in the step 3 is 2:1.
and (5) after the centrifugal washing in the step (4), washing for 3 times by using deionized water, and then, centrifugally washing for 3 times by using ethanol.
The molar ratio of thioacetamide to tungsten hexachloride in the step 5 is 5:1.
the stirring time in the step 5 is 10-60min.
The filling ratio of the step 5 is controlled to be 30-60%.
And the step 6 is repeated for 4 to 6 times.
Compared with the prior art, the invention has the following beneficial technical effects:
according to the invention, through a simple normal-temperature liquid-phase synthesis method, methylimidazole and tungsten hexachloride are oxidized in a methanol solution to obtain tungsten trioxide with uniform appearance and small size, and then WS is obtained through liquid-phase vulcanization 2 . In the process, the uniform morphology and the small size of the tungsten trioxide are ensured, so that the hydrangeal tungsten disulfide with uniform size is formed. It has large specific surface area, and is favorable for the infiltration of electrolyte and ions when used as an electrode material in the process of charging and dischargingTo be transmitted. And a large number of gaps exist in the self-assembled three-dimensional embroidered spherical structure, so that the volume expansion of the electrode material in the charging and discharging processes can be effectively relieved, and the good structural stability is kept. The preparation method is simple and easy to operate, the process parameters are easy to control, the application range is wide, the reaction time is greatly shortened, the reaction efficiency is improved, the repeatability is high, and the yield is high.
The three-dimensional embroidered spherical tungsten disulfide material prepared by the invention has uniform appearance, high electrochemical performance and stability and great application prospect in the application of sodium ion battery cathodes.
Drawings
Figure 1 is an X-ray diffraction (XRD) pattern of the three-dimensionally embroidered spherical tungsten disulfide material prepared in example 3.
FIG. 2 is a Scanning Electron Microscope (SEM) photograph of the embroidered spherical tungsten disulfide material prepared in example 3, wherein (a) is 20K, and (b) is 50K.
Fig. 3 is a graph showing the cycle performance and the rate performance of (a) the three-dimensional embroidered spherical tungsten disulfide material prepared in example 3.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
The invention relates to a three-dimensional embroidered spherical WS 2 A method of making a material comprising the steps of:
the method comprises the following steps: adding 0.3965-1.965 g of methylimidazole into 20-100 mL of methanol solvent, and stirring and dissolving to obtain a solution A;
step two: adding 0.793-3.96 g of tungsten hexachloride into 20-100 mL of methanol solvent to ensure that the molar concentration of the tungsten hexachloride is 0.1mlo/L, and stirring until the tungsten hexachloride is dissolved to obtain a solution B;
wherein the volume ratio of the methanol solution obtained in the step 1 and the step 2 is 1:1;
step three: pouring the solution B into the solution A to obtain a mixed solution C (the mass ratio of the added tungsten hexachloride to the methylimidazole is 2;
step four: washing the blue turbid liquid by using deionized water for 3 times after centrifugal washing, and then obtaining a blue precursor after centrifugal washing by using ethanol for 3 times;
step five: dispersing the precursor in an ethanol solvent, adding 0.7511-3.75 g thioacetamide (the molar ratio of the thioacetamide to the tungsten hexachloride is 5); transferring the solution into a hydrothermal kettle, controlling the filling ratio to be 30-60%, then sealing the hydrothermal kettle, putting the hydrothermal kettle into a homogeneous reaction instrument, controlling the solvothermal temperature to be 180-240 ℃, reacting for 12-72h, and naturally cooling to room temperature after the reaction is finished;
step six: opening the reaction kettle, taking out the product, repeatedly washing the product for 4 to 6 times by adopting absolute ethyl alcohol and deionized water in sequence, centrifugally separating the product, and drying the product in a freeze dryer with the vacuum degree of 10 to 40Pa for 8 to 12 hours at the temperature of between 40 ℃ below zero and 70 ℃ below zero to obtain the black embroidered spherical WS 2 A material.
Example 1:
the method comprises the following steps: adding 0.3965g of methylimidazole into 20mL of methanol solvent, and stirring until the methylimidazole is dissolved to obtain a clear and transparent solution A;
step two: adding 0.793g of tungsten hexachloride into 20mL of methanol solvent so that the molar concentration of the tungsten hexachloride is 0.1mlo/L, and stirring until the tungsten hexachloride is dissolved to obtain a clear yellow solution B;
step three: and pouring the solution B into the solution A to obtain a mixed solution C, stirring until the mixed solution C becomes a blue turbid liquid, and standing for 24 hours.
Step four: centrifugally washing the blue turbid liquid, washing the blue turbid liquid for 3 times by deionized water, and then washing the blue turbid liquid for 3 times by ethanol to obtain a blue precursor;
step five: the precursor was dispersed in ethanol solvent and 0.7511g thioacetamide was added so that the molar ratio of thioacetamide to tungsten hexachloride was 5:1, stirring for 10 min; transferring the mixture into a hydrothermal kettle, controlling the filling ratio to be 30%, then sealing the hydrothermal kettle, putting the hydrothermal kettle into a homogeneous reaction instrument, controlling the solvothermal temperature to be 180 ℃, reacting for 12 hours, and naturally cooling to room temperature after the reaction is finished.
Step six: and opening the reaction kettle, taking out the product, sequentially washing by using absolute ethyl alcohol and deionized water, carrying out centrifugal separation, repeatedly washing for 4 times, and drying in a freeze dryer at the temperature of-40 ℃ and the vacuum degree of 10Pa for 8 hours to obtain the black three-dimensional hydrangeal tungsten disulfide material.
Example 2
The method comprises the following steps: adding 1.965g of methylimidazole into 100mL of methanol solvent, and stirring until the methylimidazole is dissolved to obtain a clear and transparent solution A;
step two: adding 3.96g of tungsten hexachloride into 100mL of methanol solvent to ensure that the molar concentration of the tungsten hexachloride is 0.1mlo/L, and stirring until the tungsten hexachloride is dissolved to obtain a clear yellow solution B;
step three: and pouring the solution B into the solution A to obtain a mixed solution C, stirring until the mixed solution C becomes a blue turbid solution, and standing for 72 hours.
Step four: centrifugally washing the blue turbid liquid, washing the blue turbid liquid for 3 times by deionized water, and then washing the blue turbid liquid for 3 times by ethanol to obtain a blue precursor;
step five: dispersing the precursor in an ethanol solvent, and adding 3.75g of thioacetamide to obtain a mixture of thioacetamide and tungsten hexachloride with the molar ratio of 5:1, stirring for 60 min; transferring the mixture into a hydrothermal kettle, controlling the filling ratio to be 60%, sealing the hydrothermal kettle, putting the hydrothermal kettle into a homogeneous reaction instrument, controlling the solvothermal temperature to be 240 ℃ and the reaction time to be 72h, and naturally cooling the mixture to room temperature after the reaction is finished.
Step six: and opening the reaction kettle, taking out the product, sequentially washing by using absolute ethyl alcohol and deionized water, carrying out centrifugal separation, repeatedly washing for 6 times, and drying in a freeze dryer at the temperature of-70 ℃ and the vacuum degree of 40Pa for 12 hours to obtain the black three-dimensional hydrangeal tungsten disulfide material.
Example 3
The method comprises the following steps: adding 0.595g of methylimidazole into 30mL of methanol solvent, and stirring until the methylimidazole is dissolved to obtain a clear and transparent solution A;
step two: adding 1.19g of tungsten hexachloride into 30mL of methanol solvent to ensure that the molar concentration of the tungsten hexachloride is 0.1mlo/L, and stirring until the tungsten hexachloride is dissolved to obtain a clear yellow solution B;
step three: and pouring the solution B into the solution A to obtain a mixed solution C, stirring until the mixed solution C becomes a blue turbid solution, and standing for 12 hours.
Step four: centrifugally washing the blue turbid liquid, washing the blue turbid liquid for 3 times by deionized water, and then washing the blue turbid liquid for 3 times by ethanol to obtain a blue precursor;
step five: the precursor was dispersed in ethanol solvent, and 1.13g of thioacetamide was added so that the molar ratio of thioacetamide to tungsten hexachloride was 5:1, stirring for 60 min; transferring the mixture into a hydrothermal kettle, controlling the filling ratio to be 60%, then sealing the hydrothermal kettle, putting the hydrothermal kettle into a homogeneous reaction instrument, controlling the solvothermal temperature to be 200 ℃, reacting for 24 hours, and naturally cooling to room temperature after the reaction is finished.
Step six: and opening the reaction kettle, taking out a product, washing the product by using absolute ethyl alcohol and deionized water in sequence, performing centrifugal separation, repeatedly washing for 6 times, and drying the product in a freeze dryer at the temperature of-40 ℃ and the vacuum degree of 25Pa for 12 hours to obtain the black three-dimensional embroidered spherical tungsten disulfide material.
Fig. 1 is an X-ray diffraction (XRD) pattern of the three-dimensional embroidered spherical tungsten disulfide material prepared in example 3. The sample has the same structure with the tungsten disulfide of a hexagonal system with JCPDS serial number of 08-0237, which shows that the tungsten disulfide prepared by the method has higher purity and no impurity phase.
Fig. 2 is a Scanning Electron Microscope (SEM) photograph of the three-dimensional spherical tungsten disulfide material prepared in example 3. It can be seen that the tungsten disulfide nanosheets assembled together form a uniform embroidered ball shape.
Fig. 3 is a cycle performance diagram of the three-dimensional spherical tungsten disulfide material prepared in example 3. It can be seen that it exhibits better stability and higher capacity.
According to the method, methylimidazole and tungsten hexachloride are oxidized in a methanol solution to obtain tungsten trioxide with uniform appearance and small size, and then, tungsten disulfide is obtained through liquid-phase vulcanization. In the process, the uniform morphology and the small size are ensured so as to form the hydrangeal tungsten disulfide with uniform size. On one hand, the electrode material has a large specific surface area, and is favorable for the infiltration of electrolyte and the transmission of ions when being used as an electrode material in the charging and discharging processes. On the other hand, a large number of gaps exist in the self-assembled three-dimensional embroidered spherical structure, so that the volume expansion of the electrode material in the charging and discharging processes can be effectively relieved, and the good structural stability is kept. The preparation method is simple and easy to operate, the process parameters are easy to control, the application range is wide, the reaction time is greatly shortened, the reaction efficiency is improved, the repeatability is high, and the yield is high.
Example 4
The method comprises the following steps: adding 0.99g of methylimidazole into 50mL of methanol solvent, and stirring until the methylimidazole is dissolved to obtain a clear and transparent solution A;
step two: adding 1.98g of tungsten hexachloride into 50mL of methanol solvent to ensure that the molar concentration of the tungsten hexachloride is 0.1mlo/L, and stirring until the tungsten hexachloride is dissolved to obtain a clear yellow solution B;
step three: and pouring the solution B into the solution A to obtain a mixed solution C, stirring until the mixed solution C becomes a blue turbid solution, and standing for 48 hours.
Step four: centrifugally washing the blue turbid liquid, washing the blue turbid liquid for 3 times by deionized water, and then washing the blue turbid liquid for 3 times by ethanol to obtain a blue precursor;
step five: dispersing the precursor in an ethanol solvent, and adding 1.88g of thioacetamide to obtain a mixture of thioacetamide and tungsten hexachloride with the molar ratio of 5:1, stirring for 30 min; transferring the mixture into a hydrothermal kettle, controlling the filling ratio at 50%, sealing the hydrothermal kettle, putting the hydrothermal kettle into a homogeneous reaction instrument, controlling the solvothermal temperature at 220 ℃ and the reaction time at 60h, and naturally cooling the mixture to room temperature after the reaction is finished.
Step six: and opening the reaction kettle, taking out the product, sequentially washing by using absolute ethyl alcohol and deionized water, carrying out centrifugal separation, repeatedly washing for 6 times, and drying in a freeze dryer at the temperature of-50 ℃ and the vacuum degree of 30Pa for 12 hours to obtain the three-dimensional black hydrangeal tungsten disulfide material.
Example 5
The method comprises the following steps: adding 1.585g of methylimidazole into 80mL of methanol solvent, and stirring until the methylimidazole is dissolved to obtain a clear and transparent solution A;
step two: adding 3.17g of tungsten hexachloride into 80mL of methanol solvent so that the molar concentration of the tungsten hexachloride is 0.1mlo/L, and stirring until the tungsten hexachloride is dissolved to obtain a clear yellow solution B;
step three: and pouring the solution B into the solution A to obtain a mixed solution C, stirring until the mixed solution C becomes a blue turbid solution, and standing for 36 hours.
Step four: centrifugally washing the blue turbid liquid, washing the blue turbid liquid for 3 times by deionized water, and then washing the blue turbid liquid for 3 times by ethanol to obtain a blue precursor;
step five: dispersing the precursor in an ethanol solvent, and adding 3g of thioacetamide to obtain a mixture with the molar ratio of thioacetamide to tungsten hexachloride being 5:1, stirring for 50 min; transferring the mixture into a hydrothermal kettle, controlling the filling ratio to be 40%, then sealing the hydrothermal kettle, putting the hydrothermal kettle into a homogeneous reaction instrument, controlling the solvothermal temperature to be 240 ℃ and the reaction time to be 36h, and naturally cooling the hydrothermal kettle to room temperature after the reaction is finished.
Step six: and opening the reaction kettle, taking out a product, washing the product by using absolute ethyl alcohol and deionized water in sequence, performing centrifugal separation, repeatedly washing for 5 times, and drying the product for 10 hours in a freeze dryer with the temperature of-40 ℃ and the vacuum degree of 40Pa to obtain the three-dimensional black hydrangeal tungsten disulfide material.
Claims (4)
1. A preparation method of a three-dimensional embroidered spherical tungsten disulfide electrode material is characterized by comprising the following steps:
the method comprises the following steps: adding 0.3965 to 1.965g of methylimidazole into 20 to 100mL of methanol solvent, and stirring and dissolving to obtain a solution A;
step two: adding 0.793 to 3.96g of tungsten hexachloride into 20 to 100mL of methanol solvent to ensure that the molar concentration of the tungsten hexachloride is 0.1mlo/L, and stirring until the tungsten hexachloride is dissolved to obtain a solution B;
wherein the volume ratio of the methanol solution obtained in the first step to the methanol solution obtained in the second step is 1:1;
step three: and pouring the solution B into the solution A to obtain a mixed solution C, stirring until the mixed solution C becomes a blue turbid solution, and standing for 12-72 hours, wherein the mass ratio of the tungsten hexachloride to the methylimidazole is 2:1;
step four: centrifugally washing the blue turbid liquid to obtain a blue precursor;
step five: dispersing the precursor in an ethanol solvent, adding 0.7511 to 3.75g of thioacetamide, and stirring; transferring the solution into a hydrothermal kettle according to a filling ratio of 30-60%, then sealing the hydrothermal kettle, putting the hydrothermal kettle into a homogeneous reaction instrument, controlling the solvent heating temperature to be 180-240 ℃, the reaction time to be 12-72h, and naturally cooling to room temperature after the reaction is finished, wherein the molar ratio of thioacetamide to tungsten hexachloride is 5:1;
step six: opening the reaction kettle, taking out a product, repeatedly washing the product by using absolute ethyl alcohol and deionized water in sequence, centrifugally separating, and drying the product in a freeze dryer with the vacuum degree of 10 to 40Pa for 8 to 12h at the temperature of-40 to-70 ℃ to obtain the black embroidered spherical WS 2 A material.
2. The preparation method of the three-dimensional embroidered spherical tungsten disulfide electrode material as claimed in claim 1, wherein: and after the centrifugal washing in the step four, washing for 3 times by using deionized water, and then, carrying out centrifugal washing for 3 times by using ethanol.
3. The preparation method of the three-dimensional embroidered spherical tungsten disulfide electrode material as claimed in claim 1, wherein: and the stirring time of the step five is 10-60min.
4. The preparation method of the three-dimensional embroidered spherical tungsten disulfide electrode material as claimed in claim 1, wherein: and sixthly, repeating the washing for 4 to 6 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110277837.0A CN113044883B (en) | 2021-03-15 | 2021-03-15 | Preparation method of three-dimensional embroidered spherical tungsten disulfide electrode material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110277837.0A CN113044883B (en) | 2021-03-15 | 2021-03-15 | Preparation method of three-dimensional embroidered spherical tungsten disulfide electrode material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113044883A CN113044883A (en) | 2021-06-29 |
| CN113044883B true CN113044883B (en) | 2022-10-14 |
Family
ID=76512477
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110277837.0A Active CN113044883B (en) | 2021-03-15 | 2021-03-15 | Preparation method of three-dimensional embroidered spherical tungsten disulfide electrode material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113044883B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114784244A (en) * | 2022-04-21 | 2022-07-22 | 陕西科技大学 | Three-dimensional hollow WS2/C composite electrode material and preparation method and application thereof |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101113021A (en) * | 2007-07-03 | 2008-01-30 | 浙江大学 | Method for preparing flower-shaped molybdenum disulfide micro-balloon |
| WO2010037498A1 (en) * | 2008-10-04 | 2010-04-08 | Bayer Materialscience Ag | Method for producing tungsten trioxide (wo3) polymer hybrid compounds |
| CN103613137A (en) * | 2013-11-08 | 2014-03-05 | 电子科技大学 | Hydrothermal synthesis method of molybdenum disulfide nano flowers |
| CN105366725A (en) * | 2014-08-29 | 2016-03-02 | 中国科学院大连化学物理研究所 | Method for hydro-thermally synthesizing MoS<2> nanoflower with sulfur-containing biological reagent as sulfur source |
| CN107804873A (en) * | 2017-11-20 | 2018-03-16 | 吉林大学 | The method of the flower-shaped molybdenum disulfide electrode material of one step Hydrothermal Synthesiss and application |
| CN108155028A (en) * | 2017-12-29 | 2018-06-12 | 安徽大学 | The preparation method of the flower-shaped molybdenum disulfide high-performance super capacitor electrode of one type |
| CN109019693A (en) * | 2018-09-27 | 2018-12-18 | 青岛科技大学 | A kind of monoclinic phase WO3The preparation method and its photocatalytic applications of nanometer cuboid |
| CN109264784A (en) * | 2018-10-30 | 2019-01-25 | 陕西科技大学 | A kind of preparation method of the flower-shaped tungsten disulfide electrode material of three-dimensional self assembly |
| CN109987631A (en) * | 2017-12-29 | 2019-07-09 | 镇江海利新材料科技有限公司 | A kind of three-dimensional flower-shaped MoS with good chemical property2The preparation of material |
| CN110482608A (en) * | 2019-09-03 | 2019-11-22 | 江苏理工学院 | A kind of flower-shaped tungsten disulfide microballoon and preparation method thereof |
| CN110577242A (en) * | 2019-10-22 | 2019-12-17 | 陕西科技大学 | Regular-hexagon nano-sheet tungsten disulfide electrode material and preparation method and application thereof |
-
2021
- 2021-03-15 CN CN202110277837.0A patent/CN113044883B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101113021A (en) * | 2007-07-03 | 2008-01-30 | 浙江大学 | Method for preparing flower-shaped molybdenum disulfide micro-balloon |
| WO2010037498A1 (en) * | 2008-10-04 | 2010-04-08 | Bayer Materialscience Ag | Method for producing tungsten trioxide (wo3) polymer hybrid compounds |
| CN103613137A (en) * | 2013-11-08 | 2014-03-05 | 电子科技大学 | Hydrothermal synthesis method of molybdenum disulfide nano flowers |
| CN105366725A (en) * | 2014-08-29 | 2016-03-02 | 中国科学院大连化学物理研究所 | Method for hydro-thermally synthesizing MoS<2> nanoflower with sulfur-containing biological reagent as sulfur source |
| CN107804873A (en) * | 2017-11-20 | 2018-03-16 | 吉林大学 | The method of the flower-shaped molybdenum disulfide electrode material of one step Hydrothermal Synthesiss and application |
| CN108155028A (en) * | 2017-12-29 | 2018-06-12 | 安徽大学 | The preparation method of the flower-shaped molybdenum disulfide high-performance super capacitor electrode of one type |
| CN109987631A (en) * | 2017-12-29 | 2019-07-09 | 镇江海利新材料科技有限公司 | A kind of three-dimensional flower-shaped MoS with good chemical property2The preparation of material |
| CN109019693A (en) * | 2018-09-27 | 2018-12-18 | 青岛科技大学 | A kind of monoclinic phase WO3The preparation method and its photocatalytic applications of nanometer cuboid |
| CN109264784A (en) * | 2018-10-30 | 2019-01-25 | 陕西科技大学 | A kind of preparation method of the flower-shaped tungsten disulfide electrode material of three-dimensional self assembly |
| CN110482608A (en) * | 2019-09-03 | 2019-11-22 | 江苏理工学院 | A kind of flower-shaped tungsten disulfide microballoon and preparation method thereof |
| CN110577242A (en) * | 2019-10-22 | 2019-12-17 | 陕西科技大学 | Regular-hexagon nano-sheet tungsten disulfide electrode material and preparation method and application thereof |
Non-Patent Citations (3)
| Title |
|---|
| "二硫化钼纳米材料的制备及其光催化性能的研究";严仁杰;《中国优秀博硕士学位论文全文数据库（硕士） 工程科技I辑》;20160415(第04其、期);第27页第3.2.2节、第31页第2段及图3.6 * |
| 水热法制备不同形貌二硫化钼及其电化学电容性能;武子茂等;《兰州理工大学学报》;20161015;第42卷(第05期);第18-22页 * |
| 高温自加压制备纳米二硫化钨;赵鹏等;《无机盐工业》;20090310;第41卷(第03期);第17-18、61页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113044883A (en) | 2021-06-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Hou et al. | One-pot synthesized molybdenum dioxide–molybdenum carbide heterostructures coupled with 3D holey carbon nanosheets for highly efficient and ultrastable cycling lithium-ion storage | |
| Qiu et al. | Current progress in black phosphorus materials and their applications in electrochemical energy storage | |
| Qu et al. | Graphene oxides-guided growth of ultrafine Co3O4 nanocrystallites from MOFs as high-performance anode of Li-ion batteries | |
| CN113675408B (en) | MoS for high-performance potassium ion battery 2 /Ti 3 C 2 Preparation method of MXene composite material | |
| CN108423711B (en) | Tetragonal phase NaV2O5·H2O nano flaky powder and preparation method and application thereof | |
| CN109734132B (en) | Method for controlling synthesis of molybdenum disulfide particles in mixed solvent system | |
| WO2022032744A1 (en) | Nbs2/mxene composite material and preparation method therefor | |
| Chen et al. | Chemical reaction controlled synthesis of Cu 2 O hollow octahedra and core–shell structures | |
| KR20190095471A (en) | Graphene / 3-component material composite used in lithium ion batteries and product manufactured therefrom | |
| Zhang et al. | Zn 2 SiO 4 urchin-like microspheres: controlled synthesis and application in lithium-ion batteries | |
| CN107359328A (en) | A kind of preparation method of lithium ion battery botryoidalis niobium oxide/carbon composite electrode material | |
| CN110474034B (en) | Nitrogen-doped porous nanosheet silicon-carbon composite material and preparation method and application thereof | |
| CN109449411B (en) | Method for synthesizing tungsten disulfide @ C composite electrode material in limited domain | |
| Li et al. | 2D interspace confined growth of ultrathin MoS 2-intercalated graphite hetero-layers for high-rate Li/K storage | |
| CN107863522A (en) | Tin/the preparation method of redox graphene nano composite material, negative electrode of lithium ion battery, lithium ion battery | |
| Liang et al. | Research progress on Na3V2 (PO4) 2F3-based cathode materials for sodium-ion batteries | |
| CN109264784B (en) | Preparation method of three-dimensional self-assembled flower-shaped tungsten disulfide electrode material | |
| CN110931741A (en) | Tin sulfide quantum dot loaded titanium carbide composite nano material and preparation method thereof | |
| CN113044883B (en) | Preparation method of three-dimensional embroidered spherical tungsten disulfide electrode material | |
| CN113206244A (en) | Preparation method of vanadium nitride @ nitrogen-doped carbon as electrode material of lithium/zinc ion battery | |
| CN108511711A (en) | A kind of laminated structure vanadium phosphate sodium composite positive pole and preparation method thereof | |
| CN109037623B (en) | Positive electrode material of magnesium secondary battery and preparation method thereof | |
| CN107959024B (en) | Flaky Sb for sodium ion battery cathode2Se3Method for preparing nanocrystalline | |
| CN109449410B (en) | Preparation method of nitrogen and sulfur co-doped tungsten disulfide sodium ion battery negative electrode material | |
| Ma et al. | Yolk–shell structured metal oxide@ carbon nanoring anode boosting performance of lithium-ion batteries |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |